WO2012123731A1 - Prélecture optique destinée à déterminer une plage du rapport masse/charge - Google Patents

Prélecture optique destinée à déterminer une plage du rapport masse/charge Download PDF

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Publication number
WO2012123731A1
WO2012123731A1 PCT/GB2012/050546 GB2012050546W WO2012123731A1 WO 2012123731 A1 WO2012123731 A1 WO 2012123731A1 GB 2012050546 W GB2012050546 W GB 2012050546W WO 2012123731 A1 WO2012123731 A1 WO 2012123731A1
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WIPO (PCT)
Prior art keywords
analysis
mass
ions
generation
interest
Prior art date
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Ceased
Application number
PCT/GB2012/050546
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English (en)
Inventor
Martin Raymond Green
Jason Lee Wildgoose
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Micromass UK Ltd
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Micromass UK Ltd
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Filing date
Publication date
Application filed by Micromass UK Ltd filed Critical Micromass UK Ltd
Priority to EP12715711.3A priority Critical patent/EP2686866A1/fr
Priority to US14/004,520 priority patent/US9190251B2/en
Priority to CA2829844A priority patent/CA2829844C/fr
Priority to JP2013558503A priority patent/JP6040174B2/ja
Publication of WO2012123731A1 publication Critical patent/WO2012123731A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/004—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0027—Methods for using particle spectrometers
    • H01J49/0031—Step by step routines describing the use of the apparatus
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/004—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn
    • H01J49/0045—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn characterised by the fragmentation or other specific reaction
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/004—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn
    • H01J49/0081—Tandem in time, i.e. using a single spectrometer
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/40—Time-of-flight spectrometers

Definitions

  • the present invention relates to a mass spectrometer and a method of mass spectrometry.
  • Tandem mass spectrometry such as tandem quadrupole ("QqQ") and quadrupole
  • Time of Flight (“QToF") mass spectrometers have proved to be an invaluable tool in many applications. Tandem quadrupole instruments, in particular, have found roles in screening applications using semi targeted analyses such as parent or precursor ion scans and neutral loss scans. These types of analyses typically involve fragmenting ions exiting a scanning mass to charge ratio mass filter and using a second mass to charge ratio mass filter to target a particular fragment ion or fragment loss. As the first step of mass analysis is via a scanning mass filter, the duty cycle, and consequently the sensitivity, is reduced depending on the resolution of the mass filter and the mass to charge ratio range scanned.
  • the transmission characteristics of a mass to charge ratio mass filter can be approximated as having a uniform profile of width W Da, wherein the value of W is related to the instrument resolution.
  • W mass to charge ratio range to be scanned
  • the mass filter scanning speed is denoted as Sp Da/s
  • the length of time spent scanning across any particular mass to charge ratio is given by W/Sp (s) and the time spent for the full range scan is given by Rg/Da (s).
  • the duty cycle is therefore given by (W/Sp)/(Rg/Sp) which simplifies to W/Rg.
  • a method of Automatic Gain Control involves automatically controlling the number of ions entering a mass analyser by performing a pre-scan to determine the Total Ion Charge ("TIC"). An ion injection time is then calculated for the analytical scan based upon the determination of the Total Ion Charge. This approach prevents space charge saturation of the mass analyser.
  • a method spectrometry comprising: performing a first analysis of a sample of ions wherein one or more parameters are scanned and/or ions are sorted according to one or more parameters during the first analysis;
  • the first analysis and the second analysis may be performed using the same first analytical device.
  • the first analytical device is operated at a first resolution to perform the first analysis and is then operated at a second higher resolution to perform the second analysis.
  • the first analysis may be performed using a first analytical device and the second analysis may be performed using a second different analytical device.
  • the first analytical device is operated at a first resolution to perform the first analysis and the second analytical device is operated at a second higher resolution to perform the second analysis.
  • the parameter may comprise the mass or mass to charge ratio of the ions.
  • the first analytical device and/or the second analytical device comprise a mass analyser.
  • the first analysis preferably comprises the mass analysis of parent ions and wherein the second analysis preferably comprises the mass analysis of similar parent ions.
  • the first analysis may alternatively comprise the mass analysis of first generation, second generation, third generation or subsequent generation fragment ions and the second analysis may comprise the mass analysis of similar first generation, second generation, third generation or subsequent generation fragment ions.
  • the parameter may comprise ion mobility.
  • the first analytical device and/or the second analytical device comprise an ion mobility spectrometer.
  • the parameter may comprise collision energy.
  • the parameter comprises ionisation energy or Electron Impact ionisation energy.
  • the parameter may comprise Electron Transfer Dissociation conditions such as the mixing or reaction time between reagent anions and analyte cations (e.g. in an Electron Transfer Dissociation fragmentation device).
  • the second analysis is preferably restricted to one or more of the ranges of interest of the one or more parameters by filtering out ions having values of the one or more parameters which fall outside the one or more ranges of interest.
  • the second analysis is preferably substantially similar to the first analysis.
  • the ions analysed during the second analysis are preferably substantially similar to the ions analysed during the first analysis. Restricting the second analysis to analysing ions having one or more ranges of interest of the one or more parameters preferably has the effect of increasing the duty cycle.
  • a mass spectrometer comprising:
  • control system arranged and adapted:
  • the first analysis preferably comprises the mass analysis of parent ions and wherein the second analysis preferably comprises the mass analysis of similar parent ions.
  • the first analysis preferably comprises the mass analysis of first generation, second generation, third generation or subsequent generation fragment ions and the second analysis preferably comprises the mass analysis of similar first generation, second generation, third generation or subsequent generation fragment ions.
  • a mass spectrometer comprising:
  • control system arranged and adapted:
  • the preferred embodiment relates to methods and benefits of configuring tandem mass spectrometers so as to provide improved duty cycle for scanning devices such as quadrupoles.
  • semi targeted experiments such as precursor or parent ion scanning or neutral loss scanning the use of a fast and sensitive low resolution pre-scan can serve to restrict the mass to charge ratio range over which the analytical scan is performed resulting in improved speeds and/or an improved duty cycle.
  • a mass spectrometer comprising:
  • the mass spectrometer may comprise a tandem mass spectrometer such as a tandem quadrupole or a quadrupole Time of Flight mass analyser.
  • the first mode of operation may be a scanning or stepped quadrupole, a Time of Flight mass analyser, a magnetic sector or an ion trap.
  • the second mode of operation may be a scanning or stepped quadrupole, a Time of Flight mass analyser, a magnetic sector or an ion trap.
  • the second mode of operation may be an m/z correlated analytical approach such as ion mobility separation.
  • the fragmentation process may be via CID, SID, ETD or another dissociation process.
  • a scanning quadrupole may also act as an ion trap mass analyser or an axial Time of Flight mass analyser.
  • the fragmentation device may have an axial field or travelling wave to help maintain the fidelity of the pre-separation.
  • ions may be passed back upstream and perform the same tasks.
  • the reduced m/z range results in improved duty cycle and speed and can improve other aspects such as resolution.
  • the reduced m/z range results in improved duty cycle and speed or could improve another aspect such as mass accuracy.
  • Quantitative information can be retrieved from the pre-scan allowing the
  • the mass spectrometer may have more than two stages of fragmentation (MS n ). It is recognised that many instrument parameters may be optimised from prior knowledge of the mass range or mass ranges. These include transmission windows for RF devices, collision energy parameters and ion-ion reaction times.
  • an ion source selected from the group consisting of: (i) an Electrospray ionisation (“ESI”) ion source; (ii) an Atmospheric Pressure Photo lonisation (“APPI”) ion source; (iii) an Atmospheric Pressure Chemical lonisation (“APCI”) ion source; (iv) a Matrix Assisted Laser Desorption lonisation (“MALDI”) ion source; (v) a Laser Desorption lonisation (“LDI”) ion source; (vi) an Atmospheric Pressure lonisation (“API”) ion source; (vii) a Desorption lonisation on Silicon (“DIOS”) ion source; (viii) an Electron Impact ("El”) ion source; (ix) a Chemical lonisation (“CI”) ion source; (x) a Field lonisation (“Fl”) ion source; (xi) a Field Desorption (“FD”) ion source; (xxi
  • Atmospheric Pressure Matrix Assisted Laser Desorption lonisation ion source (xviii) a Thermospray ion source; (xix) an Atmospheric Sampling Glow Discharge lonisation (“ASGDI”) ion source; and (xx) a Glow Discharge (“GD”) ion source; and/or
  • ETD Electron Capture Dissociation
  • ECD Electron Capture Dissociation
  • PID Photo Induced Dissociation
  • PID Photo Induced Dissociation
  • a Laser Induced Dissociation fragmentation device an infrared radiation induced dissociation device
  • an ultraviolet radiation induced dissociation device an ultraviolet radiation induced dissociation device
  • a nozzle-skimmer interface fragmentation device an in-source fragmentation device
  • an in-source Collision Induced Dissociation fragmentation device (xiii) a thermal or temperature source fragmentation device
  • xiv an electric field induced fragmentation device
  • xv a magnetic field induced fragmentation device
  • an enzyme digestion or enzyme degradation fragmentation device an ion-ion reaction fragmentation device
  • an ion-molecule reaction fragmentation device an enzyme digestion or enzyme degradation fragmentation device
  • a mass analyser selected from the group consisting of: (i) a quadrupole mass analyser; (ii) a 2D or linear quadrupole mass analyser; (iii) a Paul or 3D quadrupole mass analyser; (iv) a Penning trap mass analyser; (v) an ion trap mass analyser; (vi) a magnetic sector mass analyser; (vii) Ion Cyclotron Resonance ("ICR”) mass analyser; (viii) a Fourier Transform Ion Cyclotron Resonance (“FTICR”) mass analyser; (ix) an electrostatic or orbitrap mass analyser; (x) a Fourier Transform electrostatic or orbitrap mass analyser; (xi) a Fourier Transform mass analyser; (xii) a Time of Flight mass analyser; (xiii) an orthogonal acceleration Time of Flight mass analyser; and (xiv) a linear acceleration Time of Flight mass analyser; and/or
  • (I) a device for converting a substantially continuous ion beam into a pulsed ion beam.
  • the mass spectrometer may further comprise either:
  • a C-trap and an orbitrap (RTM) mass analyser comprising an outer barrel-like electrode and a coaxial inner spindle-like electrode, wherein in a first mode of operation ions are transmitted to the C-trap and are then injected into the orbitrap (RTM) mass analyser and wherein in a second mode of operation ions are transmitted to the C-trap and then to a collision cell or Electron Transfer Dissociation device wherein at least some ions are fragmented into fragment ions, and wherein the fragment ions are then transmitted to the C-trap before being injected into the orbitrap (RTM) mass analyser; and/or
  • a stacked ring ion guide comprising a plurality of electrodes each having an aperture through which ions are transmitted in use and wherein the spacing of the electrodes increases along the length of the ion path, and wherein the apertures in the electrodes in an upstream section of the ion guide have a first diameter and wherein the apertures in the electrodes in a downstream section of the ion guide have a second diameter which is smaller than the first diameter, and wherein opposite phases of an AC or RF voltage are applied, in use, to successive electrodes.
  • Fig. 1 shows a mass spectrometer according to an embodiment of the present invention wherein a fast analyser is provided downstream of a mass filter;
  • Fig. 2 shows a mass spectrometer according to an alternative embodiment wherein a fast analyser is provided upstream of a mass filter;
  • Fig. 3 shows a mass spectrometer according to an alternative embodiment wherein ions may be switched between a mass filter and a fast analyser
  • Fig. 4 shows a mass spectrometer according to a further embodiment wherein ions pass to a device which may operate either as a mass filter and/or a fast analyser;
  • Fig. 5 shows a precursor ion scan according to an embodiment of the present invention.
  • an ion source 1 is provided upstream of a mass filtering device 2 and a low resolution high sensitivity fast analyser 3.
  • a fragmentation or dissociation device 4 may optionally be provided downstream of the low resolution high sensitivity fast analyser 3.
  • a mass analyser 5 is arranged downstream of the fragmentation or dissociation device 4 and the low resolution high sensitivity fast analyser 3.
  • ions from the ion source 1 are arranged to pass through the mass filtering device 2 which is preferably operated in a non-filtering or wide mass to charge ratio range transmission mode.
  • the ions are then onwardly transmitted to the low resolution high sensitivity fast analyser 3.
  • a fast low resolution pre-scan of the ions is then performed by the low resolution high sensitivity fast analyser 3.
  • the ions then pass on to the fragmentation or dissociation device 4 and are fragmented in the fragmentation or dissociation device 4.
  • the characteristics of the fragmentation or dissociation device 4 are preferably such that the separation achieved in the low resolution high sensitivity fast analyser 3 is preferably maintained during the fragmentation and transport process.
  • Appropriate fragment ions are then preferably analysed by the mass analyser 5 to produce a low resolution precursor ion or neutral loss scan.
  • Data from the low resolution scan is then used to determine the mass to charge ratio range or ranges of parent or precursor ions of interest.
  • One or more restricted mass to charge ratio range or ranges are then scanned in a standard parent or precursor ion or neutral loss scanning experiment by scanning the mass filter 2 in a mass to charge ratio filtering mode over the restricted mass to charge ratio range or ranges.
  • the low resolution high sensitivity fast analyser 3 is preferably switched so as to operate in a non mass to charge ratio separating mode of operation and hence functions as an ion guide.
  • the ion beam may pass through the mass filtering device 2 and the low resolution high sensitivity fast analyser 3 in reverse order as shown in Fig. 2.
  • ions may be switched between the mass filter 2 and the low resolution high sensitivity fast analyser 3 as shown in Fig. 3.
  • a single device 2/3 is provided which is preferably capable of functioning both as a mass filter device and as a low resolution high sensitivity fast analyser.
  • the device 2/3 may comprise a 2D linear ion trap with axial ejection as, for example, disclosed in Guna et. al. J Am Soc Mass Spectrom 2009, 20, 1 132-1 140.
  • the device 2/3 is preferably capable of operating either as a mass filter (e.g. quadrupole) or as a fast high sensitivity ion trap.
  • the scan speed can be as high as 20000 Da/s for 0.7 Da peak widths. Higher scan rates are possible with some loss in resolution.
  • a scan rate of 100000 Da/s may produce peak widths of -5 Da.
  • a quadrupole scan speed of 2000 Da/sec and an ion trap mode overhead time of 5 ms for cooling and injection an attempt can be made to quantify the improvements according to the preferred embodiment.
  • Fig. 5 illustrates a precursor or parent ion scan from a neo-natal screening experiment.
  • Nine precursor or parent ions were detected in the initial low resolution scan and are displayed along the bottom of Fig. 5.
  • the low resolution scan took approximately 3 ms whilst the overhead for cooling and injection took 5 ms resulting in an overall trap experimental time of -8 ms.
  • a simple double differential and threshold peak detection resulted in the identification of multiple mass to charge ratio ranges of interest (which are displayed inverted in Fig. 5).
  • the total mass to charge ratio ranges of interest add up to -32 Da and take around 16 ms to scan (ignoring quadrupole settling times) resulting in an overall cycle time of around 24 ms which equates to a duty cycle improvement of over a factor of x6 for the mass to charge ratio range shown.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

L'invention concerne un procédé de spectrométrie de masse qui consiste à effectuer une première analyse d'un échantillon d'ions, un ou plusieurs paramètres étant lus optiquement et/ou les ions étant triés selon un ou plusieurs paramètres au cours de la première analyse. Une ou plusieurs plages d'intérêt du ou des paramètres issus de la première analyse sont ensuite automatiquement déterminées. Une seconde analyse subséquente de l'échantillon d'ions est ensuite effectuée automatiquement, qui se limite à une ou plusieurs des plages d'intérêt du ou des paramètres.
PCT/GB2012/050546 2011-03-14 2012-03-13 Prélecture optique destinée à déterminer une plage du rapport masse/charge Ceased WO2012123731A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP12715711.3A EP2686866A1 (fr) 2011-03-14 2012-03-13 Prélecture optique destinée à déterminer une plage du rapport masse/charge
US14/004,520 US9190251B2 (en) 2011-03-14 2012-03-13 Pre-scan for mass to charge ratio range
CA2829844A CA2829844C (fr) 2011-03-14 2012-03-13 Prelecture optique destinee a determiner une plage du rapport masse/charge
JP2013558503A JP6040174B2 (ja) 2011-03-14 2012-03-13 質量電荷比範囲のプレスキャン

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB1104225.6 2011-03-14
GBGB1104225.6A GB201104225D0 (en) 2011-03-14 2011-03-14 Pre scan for mass to charge ratio range
US201161481384P 2011-05-02 2011-05-02
US61/481,384 2011-05-02

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WO2012123731A1 true WO2012123731A1 (fr) 2012-09-20

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US (1) US9190251B2 (fr)
EP (1) EP2686866A1 (fr)
JP (1) JP6040174B2 (fr)
CA (1) CA2829844C (fr)
GB (2) GB201104225D0 (fr)
WO (1) WO2012123731A1 (fr)

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GB201205009D0 (en) * 2012-03-22 2012-05-09 Micromass Ltd Multi-dimensional survey scans for improved data dependent acquisitions (DDA)
US10586691B2 (en) 2013-11-12 2020-03-10 Micromass Uk Limited Method of correlating precursor and fragment ions using ion mobility and mass to charge ratio
US10615014B2 (en) 2013-11-12 2020-04-07 Micromass Uk Limited Data dependent MS/MS analysis
US9881778B2 (en) 2014-04-17 2018-01-30 Micromass Uk Limited Hybrid acquisition method incorporating multiple dissociation techniques
US8921774B1 (en) * 2014-05-02 2014-12-30 908 Devices Inc. High pressure mass spectrometry systems and methods
GB201409578D0 (en) * 2014-05-30 2014-07-16 Micromass Ltd Combined tandem mass spectrometry and ion mobility mass spectrometry
US9947518B2 (en) 2014-05-30 2018-04-17 Micromass Uk Limited Combined tandem mass spectrometry and ion mobility mass spectrometry
WO2015185934A1 (fr) 2014-06-06 2015-12-10 Micromass Uk Limited Amélioration du rapport cyclique de trajets multiples
GB201410049D0 (en) * 2014-06-06 2014-07-16 Micromass Ltd Multipath duty cycle enhancement
WO2015189605A1 (fr) 2014-06-11 2015-12-17 Micromass Uk Limited Profilage ionique avec un filtre de masse quadrupolaire à balayage
US10153150B2 (en) 2015-03-29 2018-12-11 Meridion, Llc Apparatus for mass analysis of analytes by simultaneous positive and negative ionization
US9779922B1 (en) * 2017-01-17 2017-10-03 Advion Inc. Generation of discovery ion currents and mass spectrometry and uses thereof
US10128099B1 (en) 2017-07-20 2018-11-13 Thermo Finnigan Llc Systems and methods for regulating the ion population in an ion trap for MSn scans
GB202105778D0 (en) * 2021-04-23 2021-06-09 Micromass Ltd Method to reduce measurement bias
GB202207395D0 (en) * 2022-05-20 2022-07-06 Micromass Ltd Ion mobility separators
WO2025163084A1 (fr) * 2024-01-30 2025-08-07 Bruker Switzerland Ag Appareil et procédé d'analyse d'ions

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Publication number Publication date
CA2829844A1 (fr) 2012-09-20
GB201204376D0 (en) 2012-04-25
US20140048701A1 (en) 2014-02-20
GB201104225D0 (en) 2011-04-27
CA2829844C (fr) 2019-05-14
JP6040174B2 (ja) 2016-12-07
US9190251B2 (en) 2015-11-17
GB2489093B (en) 2015-10-21
GB2489093A (en) 2012-09-19
EP2686866A1 (fr) 2014-01-22
JP2014513277A (ja) 2014-05-29

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